Purification apparatus and method

ABSTRACT

Disclosed is a purification apparatus and method. The purification apparatus includes: a mobile phase distillation part for distilling a mobile phase; a mobile phase liquefaction part for liquefying the distilled mobile phase; and a purification part disposed between the mobile phase distillation part and the mobile phase liquefaction part, for mixing the mobile phase liquefied at the mobile liquefaction part with to-be-purified material, removing impurities from the mixture through a bonded phase, and sending the impurity-removed purified material to the mobile phase distillation part.

[0001] This application claims the benefit of the Korean Application No.P2002-59519 filed on Sep. 30, 2003, which is hereby incorporated byreference.

BACKGROUND OF THE INVENTION

[0002] 1. Field of the Invention

[0003] The present invention relates to a purification apparatus, andmore particularly, to an apparatus and method for purifying organicmaterial.

[0004] 2. Discussion of the Related Art

[0005] In general, purification of organic material from a mixture isperformed by a recrystallization process, a chromatography process and asublimation process.

[0006] In the recrystallization process, a solid organic material isdissolved in an organic solvent to be made in a supersaturated state andthe supersaturated organic material is then cooled, so that puresubstances are separated in a crystalline state and impurities are leftin the solvent.

[0007] In the chromatography process, a polarity difference of a mixtureis utilized. In other words, a mixture containing impurities passesthrough a bonded phase with a high polarity, thereby separating puresubstances.

[0008] The sublimation process is used to separate substances having ahigh difference in the melding point.

[0009] In other words, a mixture is heated up to a melting point andnitrogen of mobile phase is introduced into the heated mixture tothereby separate pure substances.

[0010] However, the aforementioned purification processes of organicmaterial needs a high temperature and a lot of time depending on thematerials for purification.

[0011] Accordingly, the purification process of organic material using ahigh temperature may cause the decomposition of the organic material.

[0012] Also, the sublimation process has a disadvantage in that ifimpurities are completely removed, the recrystallization process or thechromatography process should be performed to remove the impurities.

SUMMARY OF THE INVENTION

[0013] Accordingly, the present invention is directed to a purificationapparatus and method of an organic material that substantially obviateone or more problems due to limitations and disadvantages of the relatedart.

[0014] An object of the present invention is to provide a purificationapparatus and method of an organic material capable of purifying puresubstance simply and easily.

[0015] Another object of the present invention is to provide apurification apparatus and method of an organic material having asuperior substance purification performance.

[0016] Additional advantages, objects, and features of the inventionwill be set forth in part in the description which follows and in partwill become apparent to those having ordinary skill in the art uponexamination of the following or may be learned from practice of theinvention. The objectives and other advantages of the invention may berealized and attained by the structure particularly pointed out in thewritten description and claims hereof as well as the appended drawings.

[0017] To achieve these objects and other advantages and in accordancewith the purpose of the invention, as embodied and broadly describedherein, a purification apparatus includes: a mobile phase distillationpart for distilling a mobile phase; a mobile phase liquefaction part forliquefying the distilled mobile phase; and a purification part disposedbetween the mobile phase distillation part and the mobile phaseliquefaction part, for mixing the mobile phase liquefied at the mobileliquefaction part with to-be-purified material, removing impurities fromthe mixture through a bonded phase, and sending the impurity-removedpurified material to the mobile phase distillation part.

[0018] The mobile phase distillation part includes: a flask containingthe mobile phase therein; and a heater for generating heat so as todistill the mobile phase. The mobile phase is an organic solvent.

[0019] The mobile phase liquefaction part is a reflux condenser.

[0020] The purification part comprises: a cellulose or silica thimblefor mixing the mobile phase liquefied at the mobile phase liquefactionpart with the to-be-purified material; a bonded phase for removingimpurities from the mixture of the cellulose or silica thimble; and asoxhlet for sending the purified material, in which the impurities areremoved by the bonded phase, to the mobile phase distillation part.

[0021] The bonded phase is at least one or two or more selected from thegroup consisting of silica gel, alumina, celite and activated carbon.Alternatively, the bonded phase further comprises a predeterminedthickness of a sand layer formed on upper and lower surfaces thereof.

[0022] The soxhlet sends the impurity-removed purified material to themobile phase distillation part through a capillary tube. An inlet of thecapillary tube is filled with cotton such that only the purifiedmaterial passes.

[0023] Here, the capillary tube has a predetermined region that islarger in diameter than other regions.

[0024] In another aspect of the present invention, a purificationapparatus includes: a flask for containing an organic solvent therein; aheater for distilling the organic solvent; a condenser for liquefyingthe distilled organic solvent; a cellulose thimble disposed at a lowerportion of the condenser, for mixing the organic solvent liquefied atthe mobile phase liquefaction part with to-be-purified organic material;a bonded phase disposed at a lower portion of the cellulose or silicathimble, for removing impurities from the mixture of the cellulose orsilica thimble; and a soxhlet for sending the purified material, inwhich the impurities are removed by the bonded phase, to the flask.

[0025] In a further aspect of the present invention, there is provided apurification method using a purification apparatus having a mobile phasedistillation part; a mobile phase liquefaction part; and a purificationpart disposed between the mobile phase distillation part and the mobilephase liquefaction part, for removing impurities of to-be-purifiedmaterial. The method includes the steps of: distilling a mobile-phasesolvent; liquefying the distilled solvent; mixing the liquefied solventwith the to-be-purified material; removing impurities from the mixtureusing the bonded phase; sending the purified material, in which theimpurities are removed by the bonded phase, to the mobile phasedistillation part; and extracting the purified material from the mobilephase distillation part.

[0026] It is to be understood that both the foregoing generaldescription and the following detailed description of the presentinvention are exemplary and explanatory and are intended to providefurther explanation of the invention as claimed.

BRIEF DESCRIPTION OF THE DRAWINGS

[0027] The accompanying drawings, which are included to provide afurther understanding of the invention and are incorporated in andconstitute a part of this application, illustrate embodiment(s) of theinvention and together with the description serve to explain theprinciple of the invention. In the drawing:

[0028]FIG. 1 is a view of a purification apparatus according to thepresent invention.

DETAILED DESCRIPTION OF THE INVENTION

[0029] Reference will now be made in detail to the preferred embodimentsof the present invention to achieve the objects, with examples of whichare illustrated in the accompanying drawings. Wherever possible, thesame reference numbers will be used throughout the drawings to refer tothe same or like parts.

[0030]FIG. 1 is a view of a purification apparatus according to thepresent invention.

[0031] Referring to FIG. 1, a purification apparatus of the presentinvention includes a mobile phase distillation part 1, a mobile phaseliquefaction part 2 and a purification part 3 disposed therebetween.

[0032] The mobile phase distillation part 1 distills a mobile phase, andthe mobile phase liquefaction part 2 liquefies the distilled mobilephase. The purification part 3 is disposed between the mobile phasedistillation part 1 and the mobile phase liquefaction part 2. Thepurification part 3 mixes the mobile phase liquefied at the mobileliquefaction part 2 with to-be-purified material, and impurities areremoved from the mixture by using a bonded phase. Thereafter, thepurification part 3 sends the impurity-removed, or purified material tothe mobile phase distillation part 1.

[0033] The mobile distillation part 1 is provided with a flask 90containing mobile-phase organic solvent 80 and a heater 110 generatingheat so as to distill the mobile-phase organic solvent 80. An agitationmagnet 100 is disposed at a bottom of the flask 90.

[0034] The mobile phase liquefaction part 2 is constructed with a refluxcondenser 10.

[0035] Here, the reflux condenser 10 liquefies the distilling organicsolvent 80 through cooling water and sends it to a cellulose or silicathimble 30.

[0036] The purification part 3 is generally configured to have thecellulose or silica thimble 30, a bonded phase 50 and a soxhlet 20.

[0037] The cellulose or silica thimble 30 containing solid organicmaterial to be purified mixes the organic solvent 80 liquefied at thereflux condenser 10 with the solid organic material to be purified,thereby dissolving the solid organic material.

[0038] The bonded phase 50 removes impurities from the mixture containedin the cellulose or silica thimble 30.

[0039] The bonded phase 50 can be any one selected from the groupconsisting of silica gel, alumina, celite and activated carbon. A sandlayer 70 having a predetermined thickness can be formed at upper andlower portions of the bonded phase 50.

[0040] The soxhlet 20 sends the purified material, in which theimpurities are removed by the bonded phase, to the flask 90 of themobile phase distillation part 1.

[0041] Here, the soxhlet 20 sends the impurity-removed purified materialto the flask 90 through a capillary tube 40.

[0042] An inlet of the capillary tube 40 is closed up with cotton 60 soas to pass only the purified material.

[0043] A method for purifying the organic material using thepurification apparatus constructed as above will be described below.

[0044] As shown in FIG. 1, the soxhlet 20 is first installed in a lowerportion of the reflux condenser 10, and the inlet of the capillary tube40 of the soxhlet 20 is filled with the cotton 60 so as to prevent thebonded phase 50 such as silica gel from being exhausted through thecapillary tube 40.

[0045] After laying thinly a sea sand 70 on the inlet of the capillary40, the bonded phase 50 such as silica gel or alumina, which has highpolarity, is laid to a thickness of about 3 cm on the sea sand 70.

[0046] After filling the round flask 90 with about 70 ml of methylenechloride that is the organic solvent 80, the flask 90 is packed on alower portion of the soxhlet 20.

[0047] After putting 1 g of the organic material to be purified into thecellulose or silica thimble 30, the cellulose or silica thimble 30 isput into the soxhlet 20.

[0048] Here, the organic material used is an organic material that isnot liquefied well, and it contains a metal oxide as the impurities.

[0049] Specifically, this substance cannot be removed even if arecrystallization process is used. Also, this substance is a materialthat impurities are generated as ever even if a sublimation process isused.

[0050] After an installation of the purification apparatus, the flask 90containing the organic material 80 is heated to about 100° C. using theheater 110.

[0051] If so, the organic solvent 80 contained in the flask 90 isdistilled and injected into the reflux condenser 10. Then, the distilledorganic solvent 80 is liquefied by the reflux condenser 10.

[0052] At this time, the reflux condenser 10 liquefies the distillingorganic solvent 80 using cooling water.

[0053] The liquefied organic solvent 80 is dropped into the cellulose orsilica thimble 30 of the soxhlet 20.

[0054] Accordingly; the solid organic material contained in thecellulose or silica thimble 30 is dissolved by the liquefied organicsolvent 80.

[0055] Then, if the organic solvent 80 and the dissolved organicmaterial rise up to a predetermined height in the cellulose or silicathimble 30, the organic solvent 80 changes into the mobile phase, sothat the mobile phase passed through the sea sand 70 and the bondedphase, which is constituted with silica gel, alumina, celite, activatedcarbon, etc., and is exhausted through the capillary tube 40.

[0056] At this time, the purified organic material is exhaustedtogether. The metal oxide that is an unpurified impurity is blockedsince it does not pass through the sea sand 70 and the bonded phase 50.

[0057] Here, the bonded phase 50 separates the materials using polaritydifference of the mixture.

[0058] Then, the cotton installed in the inlet of the capillary tube 40covers an opening through which the purified organic material and theorganic solvent 80 are exhausted, thereby preventing silica gel,alumina, celite and activated carbon from being exhausted through thecapillary tube 40.

[0059] The organic solvent 80 and the purified organic materialexhausted through the capillary tube 40 flow into the flask 90, which isdisposed at the lower portion and contains the organic solvent 80.

[0060] Here, the organic solvent and the purified organic material areexhausted to the flask 90 by a capillary phenomenon using a surfacetension since a predetermined portion of the capillary tube 40 is formedto have a diameter larger than other portions.

[0061] If these procedures are carried out successively, the purifiedclear organic material floats in the flask 90 after about 12 hours.

[0062] Additionally, the metal oxide that is an impurity is filtered onthe upper surface of the bonded phase 50.

[0063] Accordingly, the purified organic material can be obtained simplyand easily by filtering the organic solvent 80 contained in the flask90.

[0064] If the organic material purified in the above manner is againpurified using the sublimation process, there is an advantage that avery purified organic material can be obtained.

[0065] If the organic material constructed as above is purified by usingthe purification apparatus of the present invention, a remarkabledifference is made between an organic EL device manufactured with thepurified material and an organic EL device manufactured with theunpurified material.

[0066] A following Table 1 shows a difference between a case of usingthe purified organic material and a case of using the unpurified organicmaterial when an organic EL device has a structure of ITO (1200 Å) CuPc(250 Å) NPD (350 Å) blue light emitting layer (200 Å) Alq3 (300 Å) LiF(5 Å) Al (1000 Å). TABLE 1 Current Luminance (mA) Voltage (V) (cd/m²)C.I.E. (x, y) Unpurified 1 12.0 66.0 (0.214, 0.300) matter Purified 19.3 114.5 (0.187, 0.228) matter

[0067] As shown in Table 1, it can be seen that there is a greatdifference of the luminance and the chromaticity coordinate (C.I.E)between the organic material purified using the soxhlet 20 and anythingelse.

[0068] Accordingly, it can be seen that the organic materialpurification using the purification apparatus of the present inventionhas a superiority since the material purification using the soxhlet 20improves a characteristic of the organic EL device.

[0069] Even solid organic materials that are not dissolved well can bepurified simply and easily since the present invention use the soxhletmethod and the liquid chromatography method at the same time.

[0070] As described above, the purification apparatus and method of thepresent invention has an excellent capability of purifying materialssimply and easily.

[0071] Further, materials can be easily purified even with a smallamount of organic solvent.

[0072] It will be apparent to those skilled in the art that variousmodifications and variations can be made in the present invention. Thus,it is intended that the present invention covers the modifications andvariations of this invention provided they come within the scope of theappended claims and their equivalents.

What is claimed is:
 1. A purification apparatus comprising: a mobilephase distillation part for distilling a mobile phase; a mobile phaseliquefaction part for liquefying the distilled mobile phase; and apurification part disposed between the mobile phase distillation partand the mobile phase liquefaction part, for mixing the mobile phaseliquefied at the mobile liquefaction part with to-be-purified material,removing impurities from the mixture through a bonded phase, and sendingthe impurity-removed purified material to the mobile phase distillationpart.
 2. The purification apparatus of claim 1, wherein the mobile phasedistillation part comprises: a flask containing the mobile phasetherein; and a heater for generating heat so as to distill the mobilephase.
 3. The purification apparatus of claim 2, wherein the mobilephase is an organic solvent.
 4. The purification apparatus of claim 1,wherein the mobile phase liquefaction part is a reflux condenser.
 5. Thepurification apparatus of claim 1, wherein the purification partcomprises: a cellulose or silica thimble for mixing the mobile phaseliquefied at the mobile phase liquefaction part with the to-be-purifiedmaterial; a bonded phase for removing impurities from the mixture of thecellulose or silica thimble; and a soxhlet for sending the purifiedmaterial, in which the impurities are removed by the bonded phase, tothe mobile phase distillation part.
 6. The purification apparatus ofclaim 5, wherein the bonded phase is at least one or two or moreselected from the group consisting of silica gel, alumina, celite andactivated carbon.
 7. The purification apparatus of claim 5, wherein thebonded phase further comprises a predetermined thickness of a sand layerformed on upper and lower surfaces thereof.
 8. The purificationapparatus of claim 5, wherein the soxhlet sends the impurity-removedpurified material to the mobile phase distillation part through acapillary tube.
 9. The purification apparatus of claim 8, wherein aninlet of the capillary tube is filled with cotton such that only thepurified material passes.
 10. A purification apparatus comprising: aflask for containing an organic solvent therein; a heater for distillingthe organic solvent; a condenser for liquefying the distilled organicsolvent; a cellulose or silica thimble disposed at a lower portion ofthe condenser, for mixing the organic solvent liquefied at the mobilephase liquefaction part with to-be-purified organic material; a bondedphase disposed at a lower portion of the cellulose or silica thimble,for removing impurities from the mixture of the cellulose or silicathimble; and a soxhlet for sending the purified material, in which theimpurities are removed by the bonded phase, to the flask.
 11. Thepurification apparatus of claim 10, wherein the condenser is a refluxcondenser.
 12. The purification apparatus of claim 10, wherein thebonded phase is at least one or two or more selected from the groupconsisting of silica gel, alumina, celite and activated carbon.
 13. Thepurification apparatus of claim 10, wherein the bonded phase furthercomprises a predetermined thickness of a sand layer formed on upper andlower surfaces thereof.
 14. The purification apparatus of claim 10,wherein the soxhlet sends the impurity-removed purified material to theflask through a capillary tube.
 15. The purification apparatus of claim14, wherein an inlet of the capillary tube is filled with cotton suchthat only the purified material passes.
 16. A purification method usinga purification apparatus having a mobile phase distillation part; amobile phase liquefaction part; and a purification part disposed betweenthe mobile phase distillation part and the mobile phase liquefactionpart, for removing impurities of to-be-purified material, the methodcomprising the steps of: distilling a mobile-phase solvent; liquefyingthe distilled solvent; mixing the liquefied solvent with theto-be-purified material; removing impurities from the mixture using thebonded phase; sending the purified material, in which the impurities areremoved by the bonded phase, to the mobile phase distillation part; andextracting the purified material from the mobile phase distillationpart.
 17. The purification method of claim 16, wherein the bonded phaseis at least one or two or more selected from the group consisting ofsilica gel, alumina, celite and activated carbon.
 18. The purificationmethod of claim 16, wherein the purified material is moved to the mobilephase distillation part by a capillary phenomenon having a difference ofa surface tension.
 19. The purification method of claim 16, wherein thepurified material is purified by a polarity difference of the mixture.